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    火花放电原子发射光谱法中数据处理技术的探究

    Exploration of Data Processing Techniques in Spark Discharge Atomic Emission Spectrometry

    • 摘要: 火花放电原子发射光谱法(SD-AES)中的数据处理包括校准曲线建立、仪器标准化、类型标准化,其中校准曲线建立和类型标准化属于仪器测量数据的校准过程,仪器标准化则是对仪器漂移(包括人员操作及环境因素影响)的校正过程,日常分析中数据漂移的一致性修正也是校正过程。在SD-AES分析体系中,校准与校正主要采用线性内插法和最小二乘法,前者适用于单点与两点修正,后者适用于三点及以上修正。两点夹逼法有效解决了缺少合适类型标准化样品的校准难题;单点类型标准化在低含量区间采用系数校准,在线性区间采用加法校准;折线法实现了宽范围类型标准化的处理。基于折线法与最小二乘法相结合的分段校准技术,改善了宽范围校准曲线的精度,增强了同基体材料校准曲线的普适性。在仪器漂移校正方面,基于加权最小二乘法的多点标准化比传统两点标准化具有更强的数据还原能力,能明显提高SD-AES分析的精密度。

       

      Abstract: Data processing in spark discharge atomic emission spectrometry (SD-AES) included the establishment of calibration curves, instrument standardization, and type standardization. Among these, the establishment of calibration curves and type standardization were classified as the calibration processes for instrument measurement data, while instrument standardization was the correction process for instrument drift (including the influences of personnel operations and environmental factors). The consistent correction of data drift in routine analysis was also regarded as a correction process. In the SD-AES analysis system, linear interpolation and least squares method were mainly adopted for calibration and correction. The former was applicable to single-point and two-point correction, while the latter was suitable for correction with three or more points. The two-point clamping method was effective in solving the calibration problem of lacking suitable type standardization samples. For single-point type standardization, coefficient calibration was adopted in the low-content range, and addition calibration was used in the linear range. The broken line method realized the processing of wide-range type standardization. The segmented calibration technology based on the combination of broken line method and least squares method improved the precision of wide-range calibration curves and enhanced the universality of calibration curves for materials with the same matrix. In terms of instrument drift correction, the multi-point standardization based on weighted least squares method had stronger data restoration capability than the traditional two-point standardization, which could significantly improve the precision of SD-AES analysis.

       

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